m-Xylylenediaminium di-aqua-bis-[di-hydrogen diphosphato(2-)]cobaltate(II) dihydrate.

In the title complex, (C8H14N2)[Co(H2P2O7)2(H2O)2]·2H2O, the Co(II) ion lies on an inversion center and is coordinated by two bidentate diphosphate ligands and two water mol-ecules in a slightly distorted octa-hedral coordination geometry. The m-xylylenediaminium cation is located on a twofold rotation axis. In the crystal, a three-dimensional supra-molecular assembly is constructed by O-H⋯O and N-H⋯O hydrogen bonds between the organic cations, complex anions and uncoordin-ated water mol-ecules.

Related literature

For applications of diphosphate compounds containing trans­ition metals, see: Erragh et al. (1998 ▶); Handizi et al. (1994 ▶); Dridi et al. (2000 ▶); Cheetham et al. (1999 ▶); Clearfield (1998 ▶). For bond-valence-sum calculations, see: Brown & Altermatt (1985 ▶). For geometrical features in related structures, see: Selmi et al. (2006a ▶,b ▶, 2009 ▶); Gharbi et al. (1994 ▶); Gharbi & Jouini (2004 ▶); Nelson et al. (2007 ▶).

Experimental

Crystal data

(C8H14N2)[Co(H2P2O7)2(H2O)2]·2H2O

M = 621.12

Monoclinic,

a = 11.933 (2) Å

b = 9.132 (4) Å

c = 21.441 (3) Å

β = 101.20 (2)°

V = 2291.8 (11) Å3

Z = 4

Ag Kα radiation

λ = 0.56087 Å

μ = 0.58 mm−1

T = 293 K

0.27 × 0.21 × 0.15 mm

Data collection

Enraf Nonius CAD4 diffractometer

7386 measured reflections

5609 independent reflections

4197 reflections with I > 2σ(I)

R int = 0.019

2 standard reflections every 120 min intensity decay: 2%

Refinement

R[F 2 > 2σ(F 2)] = 0.035

wR(F 2) = 0.090

S = 1.06

5609 reflections

167 parameters

6 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.87 e Å−3

Δρmin = −0.41 e Å−3

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1996 ▶); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶) and DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: WinGX publication routines (Farrugia, 2012 ▶).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S160053681302535X/lh5650sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681302535X/lh5650Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C8H14N2)[Co(H2P2O7)2(H2O)2]·2H2O	F(000) = 1276
Mr = 621.12	Dx = 1.800 Mg m−3
Monoclinic, C2/c	Ag Kα radiation, λ = 0.56087 Å
Hall symbol: -C 2yc	Cell parameters from 25 reflections
a = 11.933 (2) Å	θ = 9–11°
b = 9.132 (4) Å	µ = 0.58 mm−1
c = 21.441 (3) Å	T = 293 K
β = 101.20 (2)°	Prism, pink
V = 2291.8 (11) Å3	0.27 × 0.21 × 0.15 mm
Z = 4

Enraf Nonius CAD4 diffractometer	Rint = 0.019
Radiation source: fine-focus sealed tube	θmax = 28.0°, θmin = 2.2°
Graphite monochromator	h = −19→19
non–profiled ω scans	k = −2→15
7386 measured reflections	l = −2→35
5609 independent reflections	2 standard reflections every 120 min
4197 reflections with I > 2σ(I)	intensity decay: 2%

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ2(Fo2) + (0.0412P)2 + 1.174P] where P = (Fo2 + 2Fc2)/3
5609 reflections	(Δ/σ)max = 0.001
167 parameters	Δρmax = 0.87 e Å−3
6 restraints	Δρmin = −0.41 e Å−3

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq
Co1	0.2500	0.2500	0.5000	0.01705 (6)
P1	0.02843 (3)	0.22128 (4)	0.571350 (18)	0.01809 (7)
P2	−0.02421 (3)	0.29251 (4)	0.435477 (17)	0.01764 (7)
O1	0.14860 (8)	0.19560 (13)	0.56463 (5)	0.0244 (2)
O2	0.01855 (10)	0.34054 (12)	0.62180 (6)	0.0295 (2)
H2O2	0.0510	0.4153	0.6137	0.044*
O3	−0.03555 (9)	0.08962 (12)	0.58755 (6)	0.0272 (2)
O4	−0.04173 (9)	0.29279 (16)	0.50765 (6)	0.0343 (3)
O5	0.10009 (8)	0.30371 (12)	0.43469 (5)	0.02264 (19)
O6	−0.10026 (8)	0.41352 (11)	0.40494 (5)	0.0240 (2)
O7	−0.07639 (9)	0.14643 (13)	0.40722 (7)	0.0373 (3)
H7	−0.0275	0.0822	0.4135	0.056*
O1W	0.25749 (9)	0.47229 (13)	0.52445 (7)	0.0317 (3)
H1W1	0.2077 (14)	0.501 (3)	0.5446 (10)	0.050*
H2W1	0.3230 (10)	0.503 (3)	0.5427 (10)	0.050*
O2W	0.31653 (13)	0.3286 (2)	0.17868 (8)	0.0503 (4)
H1W2	0.3666 (14)	0.365 (3)	0.1596 (10)	0.050*
H2W2	0.2488 (10)	0.355 (3)	0.1618 (10)	0.050*
N1	0.20006 (11)	0.51928 (16)	0.36481 (7)	0.0286 (3)
H1A	0.1506	0.5933	0.3594	0.043*
H1B	0.2686	0.5518	0.3836	0.043*
H1C	0.1768	0.4511	0.3891	0.043*
C1	0.09999 (15)	0.3728 (2)	0.27477 (8)	0.0336 (3)
C2	0.0986 (2)	0.2211 (3)	0.27536 (10)	0.0499 (5)
H2	0.1644	0.1696	0.2929	0.060*
C3	0.0000	0.1464 (4)	0.2500	0.0578 (9)
H3	0.0000	0.0446	0.2500	0.069*
C4	0.0000	0.4479 (3)	0.2500	0.0305 (4)
H4	0.0000	0.5497	0.2500	0.037*
C5	0.20697 (16)	0.4554 (3)	0.30225 (10)	0.0477 (5)
H5A	0.2719	0.3896	0.3070	0.057*
H5B	0.2186	0.5330	0.2733	0.057*

	U11	U22	U33	U12	U13	U23
Co1	0.01044 (9)	0.01735 (11)	0.02374 (12)	0.00015 (8)	0.00423 (8)	−0.00035 (9)
P1	0.01487 (12)	0.01621 (14)	0.02461 (16)	0.00092 (10)	0.00736 (11)	0.00057 (11)
P2	0.01156 (12)	0.01553 (14)	0.02536 (16)	0.00003 (10)	0.00241 (11)	0.00060 (12)
O1	0.0148 (4)	0.0313 (5)	0.0283 (5)	0.0045 (4)	0.0073 (4)	0.0064 (4)
O2	0.0363 (6)	0.0195 (5)	0.0374 (6)	−0.0048 (4)	0.0187 (5)	−0.0060 (4)
O3	0.0217 (4)	0.0178 (4)	0.0446 (6)	−0.0032 (4)	0.0129 (4)	−0.0008 (4)
O4	0.0202 (4)	0.0539 (8)	0.0304 (6)	0.0138 (5)	0.0085 (4)	0.0100 (5)
O5	0.0124 (3)	0.0297 (5)	0.0256 (5)	−0.0013 (3)	0.0032 (3)	0.0023 (4)
O6	0.0182 (4)	0.0184 (4)	0.0339 (5)	0.0032 (3)	0.0014 (4)	0.0034 (4)
O7	0.0193 (5)	0.0182 (5)	0.0697 (9)	−0.0006 (4)	−0.0025 (5)	−0.0103 (5)
O1W	0.0178 (4)	0.0256 (5)	0.0525 (7)	−0.0017 (4)	0.0090 (5)	−0.0130 (5)
O2W	0.0372 (7)	0.0640 (11)	0.0506 (9)	−0.0005 (7)	0.0106 (7)	0.0063 (8)
N1	0.0203 (5)	0.0316 (7)	0.0327 (7)	−0.0009 (5)	0.0021 (5)	0.0041 (5)
C1	0.0308 (7)	0.0460 (10)	0.0233 (7)	0.0031 (7)	0.0037 (6)	−0.0020 (7)
C2	0.0589 (13)	0.0493 (12)	0.0396 (10)	0.0199 (10)	0.0051 (9)	0.0030 (9)
C3	0.086 (3)	0.0330 (14)	0.0521 (19)	0.000	0.0083 (18)	0.000
C4	0.0304 (10)	0.0333 (12)	0.0271 (10)	0.000	0.0041 (8)	0.000
C5	0.0262 (8)	0.0832 (17)	0.0347 (9)	−0.0055 (9)	0.0088 (7)	−0.0058 (10)

Co1—O1i	2.0695 (11)	O2W—H1W2	0.853 (9)
Co1—O1	2.0695 (11)	O2W—H2W2	0.855 (9)
Co1—O1Wi	2.0940 (15)	N1—C5	1.480 (3)
Co1—O1W	2.0940 (14)	N1—H1A	0.8900
Co1—O5	2.1044 (11)	N1—H1B	0.8900
Co1—O5i	2.1044 (11)	N1—H1C	0.8900
P1—O1	1.4873 (10)	C1—C2	1.385 (3)
P1—O3	1.5007 (12)	C1—C4	1.389 (2)
P1—O2	1.5554 (12)	C1—C5	1.501 (3)
P1—O4	1.5965 (12)	C2—C3	1.377 (3)
P2—O5	1.4901 (10)	C2—H2	0.9300
P2—O6	1.4975 (11)	C3—C2ii	1.377 (3)
P2—O7	1.5452 (13)	C3—H3	0.9300
P2—O4	1.6012 (13)	C4—C1ii	1.389 (2)
O2—H2O2	0.8200	C4—H4	0.9300
O7—H7	0.8200	C5—H5A	0.9700
O1W—H1W1	0.843 (9)	C5—H5B	0.9700
O1W—H2W1	0.849 (9)
O1i—Co1—O1	180.0	P2—O5—Co1	134.09 (7)
O1i—Co1—O1Wi	93.85 (5)	P2—O7—H7	109.5
O1—Co1—O1Wi	86.15 (5)	Co1—O1W—H1W1	115.7 (17)
O1i—Co1—O1W	86.15 (5)	Co1—O1W—H2W1	114.9 (17)
O1—Co1—O1W	93.85 (5)	H1W1—O1W—H2W1	109.9 (18)
O1Wi—Co1—O1W	180.00 (8)	H1W2—O2W—H2W2	112.3 (18)
O1i—Co1—O5	91.75 (4)	C5—N1—H1A	109.5
O1—Co1—O5	88.25 (4)	C5—N1—H1B	109.5
O1Wi—Co1—O5	94.01 (5)	H1A—N1—H1B	109.5
O1W—Co1—O5	85.99 (5)	C5—N1—H1C	109.5
O1i—Co1—O5i	88.25 (4)	H1A—N1—H1C	109.5
O1—Co1—O5i	91.75 (4)	H1B—N1—H1C	109.5
O1Wi—Co1—O5i	85.99 (5)	C2—C1—C4	119.07 (19)
O1W—Co1—O5i	94.01 (5)	C2—C1—C5	120.64 (19)
O5—Co1—O5i	180.00 (5)	C4—C1—C5	120.3 (2)
O1—P1—O3	116.07 (7)	C3—C2—C1	120.2 (2)
O1—P1—O2	112.49 (7)	C3—C2—H2	119.9
O3—P1—O2	106.82 (7)	C1—C2—H2	119.9
O1—P1—O4	109.69 (6)	C2ii—C3—C2	120.6 (3)
O3—P1—O4	108.66 (7)	C2ii—C3—H3	119.7
O2—P1—O4	102.15 (7)	C2—C3—H3	119.7
O5—P2—O6	117.67 (6)	C1ii—C4—C1	120.8 (2)
O5—P2—O7	112.39 (7)	C1ii—C4—H4	119.6
O6—P2—O7	107.56 (7)	C1—C4—H4	119.6
O5—P2—O4	109.15 (7)	N1—C5—C1	111.18 (15)
O6—P2—O4	103.86 (7)	N1—C5—H5A	109.4
O7—P2—O4	105.19 (8)	C1—C5—H5A	109.4
P1—O1—Co1	136.65 (7)	N1—C5—H5B	109.4
P1—O2—H2O2	109.5	C1—C5—H5B	109.4
P1—O4—P2	132.91 (7)	H5A—C5—H5B	108.0
O3—P1—O1—Co1	132.63 (10)	O7—P2—O5—Co1	−91.76 (11)
O2—P1—O1—Co1	−103.92 (11)	O4—P2—O5—Co1	24.54 (12)
O4—P1—O1—Co1	9.04 (13)	O1i—Co1—O5—P2	175.43 (10)
O1i—Co1—O1—P1	112.8 (17)	O1—Co1—O5—P2	−4.57 (10)
O1Wi—Co1—O1—P1	−109.69 (11)	O1Wi—Co1—O5—P2	81.45 (10)
O1W—Co1—O1—P1	70.31 (11)	O1W—Co1—O5—P2	−98.55 (10)
O5—Co1—O1—P1	−15.56 (11)	O5i—Co1—O5—P2	−39 (100)
O5i—Co1—O1—P1	164.44 (11)	C4—C1—C2—C3	1.9 (3)
O1—P1—O4—P2	23.46 (15)	C5—C1—C2—C3	−179.98 (16)
O3—P1—O4—P2	−104.38 (13)	C1—C2—C3—C2ii	−0.95 (14)
O2—P1—O4—P2	142.97 (12)	C2—C1—C4—C1ii	−0.93 (14)
O5—P2—O4—P1	−38.26 (15)	C5—C1—C4—C1ii	−179.09 (18)
O6—P2—O4—P1	−164.55 (12)	C2—C1—C5—N1	−104.4 (2)
O7—P2—O4—P1	82.55 (13)	C4—C1—C5—N1	73.8 (2)
O6—P2—O5—Co1	142.47 (8)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2O2···O6iii	0.82	1.74	2.5574 (18)	172
O7—H7···O3iv	0.82	1.74	2.5268 (18)	160
O1W—H1W1···O6iii	0.84 (1)	1.99 (1)	2.8289 (17)	174 (2)
O1W—H2W1···O3v	0.85 (1)	1.94 (1)	2.7891 (17)	174 (2)
O2W—H1W2···O3vi	0.85 (1)	2.15 (1)	2.972 (2)	162 (2)
O2W—H2W2···O6ii	0.86 (1)	2.12 (1)	2.946 (2)	163 (2)
N1—H1A···O2iii	0.89	2.22	2.9694 (18)	142
N1—H1A···O2Wvii	0.89	2.36	2.969 (3)	126
N1—H1B···O7v	0.89	2.01	2.8893 (18)	167
N1—H1C···O5	0.89	1.99	2.8701 (19)	171

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2O2⋯O6i	0.82	1.74	2.5574 (18)	172
O7—H7⋯O3ii	0.82	1.74	2.5268 (18)	160
O1W—H1W1⋯O6i	0.84 (1)	1.99 (1)	2.8289 (17)	174 (2)
O1W—H2W1⋯O3iii	0.85 (1)	1.94 (1)	2.7891 (17)	174 (2)
O2W—H1W2⋯O3iv	0.85 (1)	2.15 (1)	2.972 (2)	162 (2)
O2W—H2W2⋯O6v	0.86 (1)	2.12 (1)	2.946 (2)	163 (2)
N1—H1A⋯O2i	0.89	2.22	2.9694 (18)	142
N1—H1A⋯O2W vi	0.89	2.36	2.969 (3)	126
N1—H1B⋯O7iii	0.89	2.01	2.8893 (18)	167
N1—H1C⋯O5	0.89	1.99	2.8701 (19)	171

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .